CN109850907A - A method of preparing hydrophobic silica - Google Patents
A method of preparing hydrophobic silica Download PDFInfo
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- CN109850907A CN109850907A CN201910158656.9A CN201910158656A CN109850907A CN 109850907 A CN109850907 A CN 109850907A CN 201910158656 A CN201910158656 A CN 201910158656A CN 109850907 A CN109850907 A CN 109850907A
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- Prior art keywords
- hydrophobic
- acid solution
- acid
- preparation
- alkoxy
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 42
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 29
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 18
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000003607 modifier Substances 0.000 claims abstract description 12
- 125000000229 (C1-C4)alkoxy group Chemical group 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 claims abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical group CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- 238000000352 supercritical drying Methods 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims 1
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 claims 1
- 238000001694 spray drying Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 230000001376 precipitating effect Effects 0.000 description 5
- -1 papermaking Substances 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 3
- 241000790917 Dioxys <bee> Species 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229940008099 dimethicone Drugs 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of methods for preparing hydrophobic silica, comprising: (1) mixes acid with hydrophobic modifier, obtain acid solution；(2) under stiring, the acid solution that step (1) obtains is added in sodium silicate aqueous solution, the pH value of system stops that acid solution is added when reaching 8.2~9.5, continues stirring 0.5~2 hour, obtains hydrophobic silica；The structural formula of the hydrophobic modifier are as follows:Wherein, R1For C1-C4 alkyl or C1-C4 alkoxy, R2For C1-C4 alkyl, R3For C1-C4 alkoxy, R4For C1-C4 alkoxy.With existing hydrophobically modified technology, method operation of the invention is more simple, without additional processing step and equipment upgrading on the basis of original precipitated silica production technology and preparation, is suitble to large-scale industrial production.
Description
Technical field
The present invention relates to a kind of methods for preparing hydrophobic silica.
Background technique
Precipitated silica (being commonly called as white carbon black) is the second largest rubber packing for being only second to carbon black, it may also be used for modeling
The fields such as material, rubber product, papermaking, coating, cosmetics and ink.Traditional precipitated silica its table during the preparation process
Face can generate a large amount of hydroxyl, and for hydrophilic material, hygroscopicity with higher, the poor compatibility with organic system is affected
Its dispersibility in organic articles.To improve its dispersibility in organic system, hydrophobic change is carried out to precipitated silica
Property is necessary.
The hydrophobically modified of existing precipitated silica usually first generates silica, then carries out hydrophobic change to silica
Property, as applicant (CN 103466644A) discloses a kind of preparation method of hydrophabic silica before this, which is characterized in that packet
Include following steps:
A, taking concentration is 1000 parts by weight of sodium silicate solution of 12-15%, is added in sodium silicate solution:
The sodium sulphate of 100-120 parts by weight stirs to obtain mixed liquor；
B, 10-15% sulfuric acid solution is added in obtained mixed liquor to react to sodium metasilicate end of reaction, to reaction system
1200-1500 revs/min of lasting stirring, while the dimethicone of 0.1-0.2 parts by weight is added dropwise, there is sediment in reaction system；
C, by the still aging 4-5h of obtained sediment, filters pressing is then carried out, filter cake is obtained；
D, it washed repeatedly with the water added with 1-2% neopelex, wash away dimethicone, then,
It is rinsed repeatedly with clear water again, it is dry, then the ground white carbon black up to polymolecularity.
Complicated operation for above-mentioned method of modifying.
Summary of the invention
In order to improve the existing more complicated deficiency of the process for preparing hydrophobic silica, the present invention provides a kind of operations
The simpler method for preparing hydrophobic silica.
To achieve the above object, The technical solution adopted by the invention is as follows:
A method of preparing hydrophobic silica, comprising:
(1) acid is mixed with hydrophobic modifier, obtains acid solution；
(2) under stiring, the acid solution that step (1) obtains is added in sodium silicate aqueous solution, the pH value of system reaches
Stop that acid solution is added when 8.2~9.5, continues stirring 0.5~2 hour, obtain hydrophobic silica；
The structural formula of the hydrophobic modifier are as follows:Wherein, R1For C1-C4 alkyl or C1-C4 alkoxy, R2
For C1-C4 alkyl, R3For C1-C4 alkoxy, R4For C1-C4 alkoxy.
Above-mentioned C1-C4 alkyl is enumerably such as: methyl, ethyl, n-propyl, isopropyl, normal-butyl, isobutyl group, tert-butyl.
Above-mentioned C1-C4 alkoxy is enumerably such as: methoxyl group, ethyoxyl, positive propoxy, isopropoxy, n-butoxy, isobutoxy,
Tert-butoxy.
Preferably, hydrochloric acid or sulfuric acid that the acid is 0.5~1.5mol/L.
Preferably, the hydrophobic modifier is three second of methyltrimethoxysilane, dimethyldimethoxysil,ne or methyl
Oxysilane.
Preferably, the concentration of hydrophobic modifier is 0.5~5wt% in the acid solution.
Preferably, at 75~95 DEG C, acid is mixed with hydrophobic modifier, stirs 10~30 minutes, obtains acid solution.
Preferably, the concentration of the sodium silicate aqueous solution is 15~40wt%.
Preferably, the modulus of the sodium metasilicate is 2.2~3.6.
It is highly preferred that the modulus of the sodium metasilicate is 2.8~3.6.
After completion of stirring, the system of step (2) is separated by solid-liquid separation for above-mentioned steps (2), and obtained solid is washed again, dry
It is dry to get arrive hydrophobic silica.
The present invention does not require the mode of stirring particularly, can use mechanical stirring, magnetic agitation or ultrasonic agitation.
The present invention does not require the mode of separation of solid and liquid particularly, can be using centrifugation, filtering and/or sedimentation.
The present invention does not require dry mode particularly, can use drying, supercritical drying, freeze-drying or spray
Mist is dry.
The utility model has the advantages that
With existing hydrophobically modified technology, method operation of the invention is more simple, produces work in original precipitated silica
Without additional processing step and equipment upgrading on the basis of skill and preparation, it is suitble to large-scale industrial production.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Sodium metasilicate (Na2O·nSiO2) modulus measured according to GB/T4209-2008.
Embodiment 1
At 75 DEG C, the sulfuric acid of methyltrimethoxysilane and 0.5mol/L are mixed after ten minutes, acid solution is obtained,
The concentration of methyltrimethoxysilane is 0.5wt%.
Under stiring, above-mentioned acid solution is added drop-wise in sodium metasilicate (modulus 3.2) aqueous solution of mass fraction 40%, is mixed
The pH value of zoarium system stops that acid solution is added dropwise when being 9.5, filters after continuing stirring 0.5 hour, filter cake is washed with water 1 time and is sunk
Shallow lake silica slurry, precipitated silica slurry normal pressure are dried to obtain hydrophobic precipitated silicon dioxide, and obtained is hydrophobic
The specific surface area of precipitated silica is 89m2/ g, 109 ° of hydrophobic contact angle.
Embodiment 2
At 85 DEG C, after dimethyldimethoxysil,ne and the mixed in hydrochloric acid of 1.5mol/L are stirred 30 minutes, it is molten to obtain acid
Liquid, the concentration of dimethyldimethoxysil,ne are 2wt%.
Under stiring, above-mentioned acid solution is added drop-wise in sodium metasilicate (modulus 3.6) aqueous solution of mass fraction 15%, is mixed
The pH value of zoarium system stops that acid solution is added dropwise when being 9, filters and is washed with water after continuing stirring 1 hour and obtains precipitating dioxy for 2 times
SiClx slurry, precipitated silica slurry vacuum drying are dried to obtain hydrophobic precipitated silicon dioxide, obtained hydrophobic precipitating two
The specific surface area of silica is 134m2/ g, 115 ° of hydrophobic contact angle.
Embodiment 3
At 95 DEG C, methyltriethoxysilane and the mixed in hydrochloric acid of 1.0mol/L are stirred after twenty minutes, acid solution is obtained,
The concentration of methyltriethoxysilane is 5wt%.
Under stiring, above-mentioned acid solution is added drop-wise in sodium metasilicate (modulus 2.8) aqueous solution of mass fraction 30%, is mixed
The pH value of zoarium system stops that acid solution is added dropwise when being 8.5, filters after continuing stirring 1.5 hours and is washed with water 3 times and is precipitated
Silica slurry, precipitated silica slurry are dried to obtain hydrophobic precipitated silicon dioxide, obtained hydrophobic precipitating two by spraying
The specific surface area of silica is 196m2/ g, 129 ° of hydrophobic contact angle.
Embodiment 4
At 85 DEG C, the sulfuric acid of methyltriethoxysilane and 1.0mol/L are mixed after ten minutes, acid solution is obtained,
The concentration of methyltriethoxysilane is 3wt%.
Under stiring, above-mentioned acid solution is added drop-wise in sodium metasilicate (modulus 2.2) aqueous solution of mass fraction 25%, is mixed
The pH value of fit system stops that acid solution is added dropwise when being 8.2, continues to filter after stirring 2 hours and be washed with water 3 times to obtain precipitating two
Silica slurry, precipitated silica slurry are freeze-dried to obtain hydrophobic precipitated silicon dioxide, obtained hydrophobic precipitating dioxy
The specific surface area of SiClx is 144m2/ g, 120 ° of hydrophobic contact angle.
Comparative example 1
Under stiring, the sulfuric acid of 1.0mol/L is added drop-wise to sodium metasilicate (modulus 2.2) aqueous solution of mass fraction 25%
In, stop that sulfuric acid is added dropwise when the pH value of mixed system is 8.2, after continuing stirring 2 hours, methyltriethoxysilane is added dropwise and (uses
Amount is added by the actual amount of embodiment 4), it is aged 3 hours, filters and be washed with water 3 times and obtain precipitated silica slurry, precipitate
Silica slurry is freeze-dried to obtain hydrophobic precipitated silicon dioxide, and the specific surface area of obtained hydrophobic precipitated silicon dioxide is
136m2/ g, 110 ° of hydrophobic contact angle.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (10)
1. a kind of method for preparing hydrophobic silica, comprising:
(1) acid is mixed with hydrophobic modifier, obtains acid solution；
(2) under stiring, the acid solution that step (1) obtains being added in sodium silicate aqueous solution, the pH value of system reaches 8.2~
Stop that acid solution is added when 9.5, continues stirring 0.5~2 hour, obtain hydrophobic silica；
The structural formula of the hydrophobic modifier are as follows:Wherein, R1For C1-C4 alkyl or C1-C4 alkoxy, R2For C1-
C4 alkyl, R3For C1-C4 alkoxy, R4For C1-C4 alkoxy.
2. according to the method described in claim 1, it is characterized by: hydrochloric acid or sulfuric acid that the acid is 0.5~1.5mol/L.
3. according to the method described in claim 1, it is characterized by: the hydrophobic modifier is methyltrimethoxysilane, two
Methyl dimethoxysilane or methyltriethoxysilane.
4. method according to claim 1 or 3, it is characterised in that: the concentration of hydrophobic modifier is 0.5 in the acid solution
~5wt%.
5. preparation method according to claim 1, it is characterised in that: at 75~95 DEG C, acid is mixed with hydrophobic modifier
It closes, stirs 10~30 minutes, obtain acid solution.
6. preparation method according to claim 1, it is characterised in that: the concentration of the sodium silicate aqueous solution be 15~
40wt%.
7. preparation method according to claim 1 or 6, it is characterised in that: the modulus of the sodium metasilicate is 2.2~3.6.
8. preparation method according to claim 7, it is characterised in that: the modulus of the sodium metasilicate is 2.8~3.6.
9. preparation method according to claim 1, it is characterised in that: after the completion of stirring, by the system solid-liquid of step (2) point
From obtained solid is washed again, dries to get hydrophobic silica is arrived.
10. preparation method according to claim 9, it is characterised in that: the mode of the separation of solid and liquid is centrifugation, filtering
And/or sedimentation；The mode of the drying is drying, supercritical drying, freeze-drying or spray drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910158656.9A CN109850907A (en) | 2019-03-01 | 2019-03-01 | A method of preparing hydrophobic silica |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910158656.9A CN109850907A (en) | 2019-03-01 | 2019-03-01 | A method of preparing hydrophobic silica |
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ID=66899763
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110539924A (en) * | 2019-07-18 | 2019-12-06 | 中山市马里奥机械科技有限公司 | Full-automatic production system of silicone adhesive |
| CN111188188A (en) * | 2020-01-14 | 2020-05-22 | 南京工业大学 | Preparation method of hydrophobic precipitated silica composite material |
| CN111777988A (en) * | 2020-05-29 | 2020-10-16 | 清华苏州环境创新研究院 | Hydrophobic material and preparation method thereof |
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| CN111777988A (en) * | 2020-05-29 | 2020-10-16 | 清华苏州环境创新研究院 | Hydrophobic material and preparation method thereof |
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